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Self-supporting through-hole alumina film preparation method

A kind of aluminum oxide film, self-supporting technology, applied in the direction of anodic oxidation, etc., can solve the problems of injury, easy pollution of the environment, personal life, long peeling time, etc., and achieve the effect of simple operation, low energy consumption and broad application prospects

Inactive Publication Date: 2008-09-17
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since this technique often uses HgCl 2 , CuCl 2 or SnCl 4 If the sample is immersed in the corrosive solution for a long time, metal impurity ions will be introduced into the aluminum oxide film, which will easily pollute the environment and even cause personal injury; the strong pulse electrochemical stripping method is often used in HClO 4 Although the peeling time is short, a higher voltage (generally 5-10V higher than the film forming voltage) is required to use the gas pressure generated by the reduction reaction to peel the aluminum oxide film from the aluminum substrate; reverse electric peeling Although the method is easy to operate, the peeling time is long (more than 12 hours), and the aluminum oxide film after peeling still retains the barrier layer, no through-hole structure is formed, and chemical etching is still required to remove the barrier layer; using argon ion bombardment technology, Sputtering along the tangential direction of the bottom of the closed hole can remove the barrier layer, but this method still needs to be pre-treated with HgCl 2 Erosion of aluminum substrate by saturated solution

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0018] In this embodiment, a self-supporting through-hole aluminum oxide film is specifically prepared according to the following steps and conditions.

[0019] (1) Pretreatment: First, the metal aluminum sheet with a thickness of 0.1 mm and a purity of 99.5% is washed in acetone and ethanol in sequence to remove surface oil, dried in the atmosphere, and then annealed at 500 ° C for 2 hours in an oxygen atmosphere ;

[0020] (2) Electrochemical polishing: the pretreated metal aluminum sheet was electrochemically polished for 3 minutes in a mixed solution of perchloric acid and ethanol with a volume ratio of 1:9, and the voltage was 15V;

[0021] (3) Anodic oxidation: the electrolytic solution is selected as 0.3M oxalic acid, and the voltage is 40V, and the polished aluminum sheet is anodized for 6 hours;

[0022] (4) Thinning the barrier layer: use the current recovery method to reduce the voltage by 1V each time, until the power is turned off after 1V;

[0023] (5) Electrol...

Embodiment 2

[0025] The process and steps of Example 1 were repeated, and the voltage was -4.5V during the electrolytic film stripping and through-hole process, and the electrolysis was performed for 10 minutes to produce a product.

Embodiment 3

[0027] The process and steps of Example 1 were repeated, and the voltage was -5V during the electrolytic stripping and through-hole process, and the electrolysis was performed for 3 minutes to produce a product.

[0028] The voltages used in the electrochemical process in the above examples are all provided by a DH1716 DC stabilized voltage and stabilized current power supply.

[0029] To above-mentioned embodiment and product thereof in conjunction with appendix figure 1 For the analysis, the electrochemically polished metal aluminum sheet is first oxidized by anodic oxidation method to form an aluminum oxide film (A) on the surface, and the barrier layer separates the porous aluminum oxide layer from the metal aluminum substrate, and its thickness satisfies the constant pressure corrosion condition A linear relationship of 1.4nm / V; secondly, the barrier layer (B) was thinned by the current recovery method. Since the thickness of the barrier layer is proportional to the anod...

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Abstract

The invention relates to a method for preparing a self-supporting through-hole alumina film by cathode electrolysis process in the neutral aqueous solution, which belongs to the physical material field. An electropolished metallic aluminum sheet is oxidated by an anodic oxidation method to form an alumina film on the surface thereof, a barrier layer separates the porous alumina film from a metallic aluminum substrate, the thickness thereof meets the linear relation of 1.4nm / V to the constant-pressure corrosion condition; the barrier layer is thinned by adopting a current reversion method, as the thickness of the barrier layer is proportional to the anode oxidation voltage, reducing the oxidation voltage gradually can effectively lower the thickness of the barrier layer, the alumina film can be peeled off by lower cathode electrolysis voltage; at last a cathode electrolysis method is adopted to electrolyze the peeled film and through holes in neutral potassium chloride aqueous solution, the self-supporting through-hole alumina film can be fully peeled off from the aluminum substrate to obtain a product. The method has the advantages of simple operation, low energy consumption, no environment pollution and so on. The product has broad prospects in the aspects of nanometer material synthesis and nanometer device application.

Description

Technical field: [0001] The invention relates to a process method for preparing an aluminum oxide film in the field of physical materials, in particular to a method for preparing a self-supporting through-hole aluminum oxide film by adopting a cathodic electrolysis process in a neutral aqueous solution. Background technique: [0002] Anodic aluminum oxide membrane (Anodic Alumina Membrane, AAM) is a nanostructure with ordered pores that grows self-organized during the anodic oxidation process. It has high aspect ratio, high order, adjustable nanopore size, and high temperature resistance. , Good insulation and other characteristics are favored by people. The use of template assembly technology to obtain nano-ordered arrays is of great significance for the development of large-scale functional devices, such as field emission devices, sensors, storage devices, and optoelectronic devices. Commonly used template synthesis methods based on porous alumina films, such as electroch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D11/04C25D11/16C25D11/10C25F3/04
Inventor 王清涛王文娟龙云泽
Owner QINGDAO UNIV
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